CN103937165A - Deep sea-using solid buoyancy material with semi-interpenetrating polymer network structure and preparation method thereof - Google Patents
Deep sea-using solid buoyancy material with semi-interpenetrating polymer network structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a deep sea-using solid buoyancy material with a semi-interpenetrating polymer network structure and a preparation method thereof. The deep sea-using solid buoyancy material comprises, by weight, 100 parts of matrix epoxy resin, 5 to 40 parts of an epoxy active diluent, 10 to 60 parts of polyurethane elastomer, 0.5 to 5 parts of aramid fiber with dopamine coatings, 20 to 60 parts of hollow glass microbead obtained via surface modification with a silane coupling agent, 5 to 20 parts of a flexibilizer, 40 to 80 parts of a curing agent, and an appropriate amount of a catalyst. The materials above are subjected to curing molding at a pressure of 20MPa, wherein curing molding is carried out at a temperature of 110 DEG C for 2h, at a temperature of 140 DEG C for 4h, and at a temperature of 160 DEG C for 4h successively. It is shown by sample detection that, compressive strength of the solid buoyancy material ranges from 80 to 140MPa, true density ranges from 0.35 to 0.52g/cm<3>, water absorption rate is less than 1.9%, the solid buoyancy material is uniform, and the preparation method is simple and is beneficial for industrialized production.
Description
Technical field
The invention belongs to nonmetal functional composite material technical field, relate in particular to a kind of deep-sea containing semi-intercrossing network solid buoyancy material and preparation method thereof.
Background technology
Solid buoyancy material is the matrix material of a kind of low density, high strength, low water absorption, is inorganic light weight packing material is filled in organic polymer material, and the class solid compounds obtaining through physical-chemical reaction.In recent years, along with the progress of Ocean Technology in China and ocean science, more and more higher for the mechanical property demand of solid buoyancy material at aspects such as oceanic resources, marine instrument and equipment, bathyscaph and petroleum pipe line coatings, traditional solid buoyancy material can not meet the demands, and therefore researching and developing the solid buoyancy material that mechanical property is higher becomes development trend.Patent CN101735566 has reported a kind of buoyancy material processed of serving the depth of water and can reach 11000 meters of depth of waters, this solid buoyancy material mainly contains multiple epoxide groups the reticulated structure closely forming through curing cross-linked and symmetrical resin structure based on high-performance epoxy resin, makes it have good solidification intensity and stable mechanical property.
Research discovery, for polymer composite material, the introducing of general topology structure, network cross-linked IPN and Semi-IPN and enhancement filler can obviously improve the mechanical property of matrix material.The people such as Rosu are at paper (Polymer degradation and stability, 2012,97:1261-1269) report by introduce urethane segment in epoxy resin-base and formed Semi-IPN network structure, thereby promoted the mechanical property of epoxy resin.Based on this, the inventor thinks and is applied to the enhancing of solid buoyancy material by inierpeneirating network structure and filler are strengthened to two kinds of means simultaneously, can further improve the ultimate compression strength of buoyancy material, thereby improves the service depth of water of buoyancy material.In the present invention, by introduce polyurethane elastomer segment and with epoxy blend curing cross-linked, obtain inierpeneirating network structure, thereby also add and introduce the deep-sea solid buoyancy material containing semi-intercrossing network that builds a kind of complex construction by the aramid fiber of Dopamine HCL coating, the aramid fiber synergy of the Dopamine HCL coating of this material based on semi-intercrossing network and enhancing itself, still belong to the first time technically, the solid buoyancy material maximum compressive strength obtaining can reach 140MPa, and method is simply easy to suitability for industrialized production and application.
Summary of the invention
The object of the invention is to: a kind of deep-sea containing semi-intercrossing network solid buoyancy material and preparation method thereof is provided, adopt the method for polymer grafting modification, in epoxy group(ing) solid buoyancy material, introduce polyurethane elastomer, make polymer network IPN each other form reticulated structure closely, realize the object that strengthens solid buoyancy material ultimate compression strength; Utilize Dopamine HCL to carry out top coat modification to aramid fiber simultaneously, improve the connectivity between aramid fiber and solid buoyancy material base material, realize the object of the mechanical property that improves solid composite material.
To achieve these goals, the present invention adopts following technical scheme:
Containing the deep-sea solid buoyancy material of semi-intercrossing network, it is characterized in that: this material prescription component is counted with weight part: 0.5～5 part of the aramid fiber of 100 parts of substrate ring epoxy resins, 5～40 parts of epoxy active diluents, 10～60 parts of polyurethane elastomers, Dopamine HCL coating, 20～60 parts of silane coupling agent surface-treated hollow glass micropearls, 5～20 parts of toughner, 40～80 parts, solidifying agent, catalyzer are appropriate.Wherein, described substrate ring epoxy resins is one or more in dihydroxyphenyl propane based epoxy resin, novolac epoxy, aliphatic epoxy resin and hydridization type epoxy resin; Described epoxy active diluent is butylglycidyl ether, 1,4-butanediol diglycidyl ether, ethylene glycol diglycidylether, phenyl glycidyl ether, polypropylene glycol diglycidyl ether, fatty glycidyl ether, benzyl glycidyl ether, 1, one or more in 6-hexanediol diglycidyl ether, propylene oxide o-cresyl ether or o-tolyl glycidyl ether, neopentylglycol diglycidyl ether.
Described method for synthesizing urethane elastomer is: by a certain amount of poly-(glycol adipate), 1,3-dihydroxyl butane and tolylene diisocyanate (three's mol ratio is 1:5:6) join in dimethyl formamide, at 80 DEG C, stirring reaction is after 4～6 hours, after removing solvent, obtain polyurethane elastomer, wherein, described vulcabond is the one in tolylene diisocyanate, diphenylmethanediisocyanate and hexamethylene diisocyanate.
Further, described poly-(glycol adipate) for molecular formula be (CH
2)
4[CO
2(CH
2cH
2o)
nh]
2, molecular weight is one or more in 100～20000.
Described aramid fiber refers to and contains a class aromatic polyamide structure and through the coating modified aramid fiber short fiber of surperficial Dopamine HCL, can be para-aramid fiber, meta-aramid fibers and containing one or more in the aramid fiber of heteroaromatic tynex heterocycle.
Further, the method of the described coating modified aramid fiber short fiber of surperficial Dopamine HCL is: it is in 0.05～2.0mg/mL dopamine hydrochloride solution that aramid fiber short fiber is joined to concentration, under room temperature, stir after 4～48 hours, filter and will after the aramid fiber short fiber cleaning-drying obtaining, obtain having the aramid fiber of Dopamine HCL coating.
Described silane coupling agent surface-treated hollow glass micropearl, the ultimate compression strength of its matrix hollow glass micropearl is 30～125MPa, real density is 0.125～0.6g/cm
3, particle diameter is 10～120 μ m, inner chamber is filled with gas or is vacuum, silane coupling agent surface treatment method is: hollow glass micropearl is added in 5～30% sodium hydroxide solution or 30% superoxol, under room temperature, stir 2～4h, filter and take out cenosphere, utilize deionized water to wash hollow glass micropearl, by the hollow glass micropearl obtaining vacuum-drying 12 hours at 80 DEG C, then join in the ethanolic soln of silane coupling agent and at room temperature stir 5～10h, finally take out and be placed in baking oven, at 80 DEG C, be dried 24～48 hours, wherein said silane coupling agent is KH-550, KH-570, KH-560, A-151, one in A-171.
Described toughner is one or more in rubber-like toughner, thermoplastic elastomer class toughner, Versamid and low molecular nonactive toughner.
Described solidifying agent be in alkaline amine curing agent, acid acid anhydride type curing agent, fatty amines, low molecular polyamides class add-on type solidifying agent or imidazole curing agent one or more.
Described catalyzer is one or more in methyl tetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride, diethylenetriamine, triethylene tetramine etc.
The preparation method of solid buoyancy material for a kind of deep-sea containing semi-intercrossing network, its concrete steps are: substrate ring epoxy resins, epoxy active diluent, polyurethane elastomer, the aramid fiber of Dopamine HCL coating, hollow glass micropearl, toughner are joined in vacuum mixer and in the vacuum mixer of 60～80 DEG C, stirred 20～30 minutes, then add solidifying agent, catalyzer continues to stir 20 minutes by gained mixture injection mould, curing molding under the pressure of 20MPa, program curing is followed successively by 110 DEG C 2 hours, at 140 DEG C 4 hours, at 160 DEG C 4 hours.
With existing deep-sea with compared with solid buoyancy material, beneficial effect of the present invention is: the method that adopts polymer grafting modification, in epoxy group(ing) solid buoyancy material, introduce polyurethane elastomer, make polymer network IPN each other form reticulated structure closely, utilize Dopamine HCL to carry out top coat modification to aramid fiber simultaneously, improve the connectivity between aramid fiber and solid buoyancy material base material, by inierpeneirating network structure and filler enhancing are applied to solid buoyancy material simultaneously, make prepared solid buoyancy material there is ultimate compression strength high, the advantage of good mechanical property.
Brief description of the drawings
Fig. 1 is the Electronic Speculum figure containing the deep-sea of semi-intercrossing network solid buoyancy material that technical solution of the present invention prepares;
Fig. 2 be the para-aramid fiber digital photograph (a) that adopts in example 1 and Dopamine HCL coating modified before the SEM figure of (c) after (b) and modification.
Embodiment
Below in conjunction with specific examples, technical scheme of the present invention is described further.
Embodiment 1
Containing a deep-sea solid buoyancy material for semi-intercrossing network, this material prescription component is counted with weight part: 2 parts of the aramid fibers of 100 parts of substrate ring epoxy resins, 10 parts of epoxy active diluents, 20 parts of polyurethane elastomers, Dopamine HCL coating, 60 parts of silane coupling agent surface-treated hollow glass micropearls, 10 parts of toughner, 40 parts, solidifying agent, 2 parts of catalyzer.
Described substrate ring epoxy resins is by bisphenol A type epoxy resin E44.
Described epoxy active diluent is BDDE.
Described method for synthesizing urethane elastomer is: will gather (glycol adipate), 1,3-dihydroxyl butane, diphenylmethanediisocyanate (three's mol ratio is 1:5:6) join in dimethyl formamide, at 80 DEG C, stirring reaction is after 4～6 hours, after removing solvent, obtain polyurethane elastomer, recording molecular weight by gel permeation chromatography (GPC) is Mn=120.000.
Described aramid fiber is para-aramid fiber (purchased from E.I.Du Pont Company), Dopamine HCL coating modified method in surface is: the short fiber that is first cut into 2～5mm length, then joining concentration is in 1.0mg/mL dopamine hydrochloride solution, under room temperature, stir after 12 hours, after filtration taking-up cleaning-drying, obtain having the para-aramid fiber of Dopamine HCL coating.
Described silane coupling agent surface-treated hollow glass micropearl, its matrix hollow glass micropearl is hollow glass micropearl K37, silane coupling agent surface-treated method is: hollow glass micropearl K37 is added in 10% sodium hydroxide solution, under room temperature, stirring a large amount of deionized waters of taking-up after 2 hours washs 10 times, at 80 DEG C, vacuum-drying is after 6 hours, join in ethanolic soln, add again silane coupling agent KH560, at 60 DEG C, stirring reaction took out after 5 hours, with after deionized water wash, in 60 DEG C of vacuum drying ovens, be dried 6 hours, obtain silane coupling agent KH560 surface-treated hollow glass micropearl.
Described toughner is acrylonitrile-butadiene-styrene copolymer (ABS).
Described solidifying agent is MALEIC ANHYDRIDE.
Described catalyzer is diethylenetriamine.
The preparation method of solid buoyancy material for a kind of deep-sea containing semi-intercrossing network, its concrete steps are: by described bisphenol A type epoxy resin E44100 part, 1, 10 parts of 4-butanediol diglycidyl ethers, molecular weight is 20 parts of the polyurethane elastomers of Mn=120.000, 2 parts of the para-aramid fibers of Dopamine HCL coating, 60 parts of silane coupling agent KH560 surface-treated hollow glass micropearls, 10 parts of acrylonitrile-butadiene-styrene copolymer (ABS) toughner join in vacuum mixer and in the vacuum mixer of 80 DEG C, stir 30 minutes, then add 40 parts of solidifying agent MALEIC ANHYDRIDE, 2 parts of continuation of divinyl-triamine catalyst are stirred and gained mixture were injected to mould in 20 minutes, curing molding under the pressure of 20MPa, program curing is followed successively by 110 DEG C 2 hours, at 140 DEG C 4 hours, deep-sea solid buoyancy material containing semi-intercrossing network after the after fixing demoulding in 4 hours at 160 DEG C.
Embodiment 2
Containing a deep-sea solid buoyancy material for semi-intercrossing network, this material prescription component is counted with weight part: 2.5 parts of the aramid fibers of 100 parts of substrate ring epoxy resins, 15 parts of epoxy active diluents, 10 parts of polyurethane elastomers, Dopamine HCL coating, 50 parts of silane coupling agent surface-treated hollow glass micropearls, 5 parts of toughner, 40 parts, solidifying agent, 2 parts of catalyzer.
Described substrate ring epoxy resins is by bisphenol A type epoxy resin E51.
Described epoxy active diluent is polypropylene glycol diglycidyl ether.
Described method for synthesizing urethane elastomer is: poly-(glycol adipate), 1,3-dihydroxyl butane and tolylene diisocyanate (three's mol ratio is 1:5:6) join in dimethyl formamide, at 80 DEG C, stirring reaction is after 4～6 hours, after removing solvent, obtain polyurethane elastomer, recording molecular weight by gel permeation chromatography (GPC) is Mn=180.000.
Described aramid fiber is aramid III fiber (gorgeous purchased from Guangdong coloured silk), Dopamine HCL coating modified method in surface is: the short fiber that is first cut into 2～5mm length, then joining concentration is in 0.5mg/mL dopamine hydrochloride solution, under room temperature, stir after 12 hours, after filtration taking-up cleaning-drying, obtain having the aramid III fiber of Dopamine HCL coating.
Described silane coupling agent surface-treated hollow glass micropearl, its matrix hollow glass micropearl is hollow glass micropearl K46, silane coupling agent surface-treated method is: hollow glass micropearl K46 is joined in 30% superoxol, under room temperature, stirring taking-up deionized water after 2 hours washs 10 times, at 80 DEG C, vacuum-drying is after 6 hours, join in ethanolic soln, add again silane coupling agent KH570, at 60 DEG C, stirring reaction took out after 5 hours, with after deionized water wash, in 60 DEG C of vacuum drying ovens, be dried 6 hours, obtain silane coupling agent KH570 surface-treated hollow glass micropearl.
Described toughner is acrylonitrile-butadiene-styrene copolymer (ABS).
Described solidifying agent is MALEIC ANHYDRIDE.
Described catalyzer is diethylenetriamine.
The preparation method of solid buoyancy material for a kind of deep-sea containing semi-intercrossing network, its concrete steps are: by described bisphenol A type epoxy resin E51100 part, 1, 15 parts of 4-butanediol diglycidyl ethers, molecular weight is 10 parts of the polyurethane elastomers of Mn=180.000, 2.5 parts of the aramid III fibers of Dopamine HCL coating, 60 parts of silane coupling agent KH570 surface-treated hollow glass micropearls, 10 parts of acrylonitrile-butadiene-styrene copolymer (ABS) toughner join in vacuum mixer and in the vacuum mixer of 80 DEG C, stir 30 minutes, then add 40 parts of solidifying agent MALEIC ANHYDRIDE, 2 parts of continuation of divinyl-triamine catalyst are stirred and gained mixture were injected to mould in 20 minutes, curing molding under the pressure of 20MPa, program curing is followed successively by 110 DEG C 2 hours, at 140 DEG C 4 hours, deep-sea solid buoyancy material containing semi-intercrossing network after the after fixing demoulding in 4 hours at 160 DEG C.
Use solid buoyancy material through sample detection at the deep-sea containing semi-intercrossing network prepared example 1,2, its performance is in table 1, and wherein density adopts U.S. army mark MIL-S-24154A to measure, and resistance to impact shock is measured according to ISO179-1-2010 standard.
Table 1-product performance index
| ? | Density (g/cm 3) | Pressure resistance (MPa) | Water-intake rate (%) |
| Embodiment 1 | 0.47 | 126 | ＜2.7 |
| Embodiment 2 | 0.52 | 140 | ＜1.9 |
Can find out from upper table, the solid buoyancy material ultimate compression strength of the deep-sea containing semi-intercrossing network that adopts technical solution of the present invention to prepare is high, and density is little, and water-intake rate is low, is a kind of deep-sea solid buoyancy material of excellence.
Claims (10)
1. containing the deep-sea solid buoyancy material of semi-intercrossing network, it is characterized in that: this material prescription component is counted with weight part: 0.5～5 part of the aramid fiber of 100 parts of substrate ring epoxy resins, 5～40 parts of epoxy active diluents, 10～60 parts of polyurethane elastomers, Dopamine HCL coating, 20～60 parts of silane coupling agent surface-treated hollow glass micropearls, 5～20 parts of toughner, 40～80 parts, solidifying agent, catalyzer are appropriate.
2. the preparation method of the deep-sea containing a semi-intercrossing network according to claim 1 use solid buoyancy material, it is characterized in that: this preparation method's concrete steps are: by substrate ring epoxy resins, epoxy active diluent, polyurethane elastomer, the aramid fiber of Dopamine HCL coating, hollow glass micropearl, toughner joins in vacuum mixer and in the vacuum mixer of 60～80 DEG C, stirs 20～30 minutes, then add solidifying agent, catalyzer continues to stir 20 minutes by gained mixture injection mould, curing molding under the pressure of 20MPa, program curing is followed successively by 110 DEG C 2 hours, at 140 DEG C 4 hours, within at 160 DEG C 4 hours, can prepare the deep-sea solid buoyancy material containing semi-intercrossing network.
3. a kind of deep-sea solid buoyancy material containing semi-intercrossing network as claimed in claim 1, is characterized in that: described substrate ring epoxy resins is one or more in dihydroxyphenyl propane based epoxy resin, novolac epoxy, aliphatic epoxy resin and hydridization type epoxy resin.
4. a kind of deep-sea solid buoyancy material containing semi-intercrossing network as claimed in claim 1, it is characterized in that: described epoxy active diluent is butylglycidyl ether, 1,4-butanediol diglycidyl ether, ethylene glycol diglycidylether, phenyl glycidyl ether, polypropylene glycol diglycidyl ether, fatty glycidyl ether, benzyl glycidyl ether, 1, one or more in 6-hexanediol diglycidyl ether, propylene oxide o-cresyl ether or o-tolyl glycidyl ether, neopentylglycol diglycidyl ether.
5. a kind of deep-sea solid buoyancy material containing semi-intercrossing network as claimed in claim 1, it is characterized in that: described method for synthesizing urethane elastomer is: by a certain amount of poly-(glycol adipate), 1,3-dihydroxyl butane, vulcabond (three's mol ratio is 1:5:6) join in dimethyl formamide, at 80 DEG C, stirring reaction is after 4～6 hours, after removing solvent, obtain polyurethane elastomer, wherein said vulcabond is the one in tolylene diisocyanate, diphenylmethanediisocyanate and hexamethylene diisocyanate; Described poly-(glycol adipate) molecular weight is one or more in 100～20000, and molecular formula is (CH
2)
4[CO
2(CH
2cH
2o)
nh]
2.
6. a kind of deep-sea containing semi-intercrossing network as claimed in claim 1 solid buoyancy material and preparation method thereof, it is characterized in that: described aramid fiber refers to the aramid fiber short fiber that contains a class aromatic polyamide structure, specifically para-aramid fiber, meta-aramid fibers and containing one or more in the aramid fiber of heteroaromatic tynex heterocycle; The coating modified method of its surperficial Dopamine HCL is that aramid fiber short fiber is joined to concentration is in 0.05～2.0mg/mL dopamine hydrochloride solution, under room temperature, stir after 4～48 hours, filter and will after the aramid fiber short fiber cleaning-drying obtaining, obtain having the aramid fiber of Dopamine HCL coating.
7. a kind of deep-sea containing semi-intercrossing network as claimed in claim 1 solid buoyancy material and preparation method thereof, it is characterized in that: described silane coupling agent surface-treated hollow glass micropearl, the ultimate compression strength of its matrix hollow glass micropearl is 30～125MPa, real density is 0.125～0.6g/cm2, particle diameter is 10～120 μ m, and inner chamber is filled with gas or is vacuum, silane coupling agent surface treatment method is: hollow glass micropearl is added in 5～30% sodium hydroxide solution or 30% superoxol, under room temperature, stir 2～4h, filter and take out cenosphere, utilize deionized water to wash hollow glass micropearl, by the hollow glass micropearl obtaining vacuum-drying 12 hours at 80 DEG C, then join in the ethanolic soln of silane coupling agent and at room temperature stir 5～10h, finally take out and be placed in baking oven, at 80 DEG C, be dried 24～48 hours, wherein said silane coupling agent is KH-550, KH-570, KH-560, A-151, one in A-171.
8. a kind of deep-sea containing semi-intercrossing network as claimed in claim 1 solid buoyancy material and preparation method thereof, is characterized in that: described toughner is one or more in rubber-like toughner, thermoplastic elastomer class toughner, Versamid and low molecular nonactive toughner.
9. a kind of solid buoyancy material and preparation method thereof for the deep-sea containing semi-intercrossing network as claimed in claim 1, is characterized in that: described solidifying agent be in alkaline amine curing agent, acid acid anhydride type curing agent, fatty amines, low molecular polyamides class add-on type solidifying agent or imidazole curing agent one or more.
10. a kind of deep-sea containing semi-intercrossing network as claimed in claim 1 solid buoyancy material and preparation method thereof, is characterized in that: described catalyzer is one or more in methyl tetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride, diethylenetriamine, triethylene tetramine etc.
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